Claims
- 1. A method for preparing a cross-bridged macropolycycle comprising a series of steps of derivatizing cyclam or a particular acyclic tetraamine, wherein said series of steps is carried out using one solvent system.
- 2. A method according to claim 1 wherein said solvent system is an alcoholic solvent system.
- 3. A method according to claim 1 wherein said solvent system comprises from about 60% to 100% of a C1-C4 alcohol or mixtures thereof.
- 4. A method according to claim 1 wherein said solvent system is ethanol or mixtures of ethanol with water.
- 5. A method according to claim 1 wherein said series of steps are all carried out in one reaction vessel.
- 6. A method for preparing a cross-bridged macropolycycle comprising a series of steps of derivatizing cyclam or a particular acyclic tetraamine including a step of quaternizing an intermediate using a quaternizing agent, wherein said step is carried out using less than fifteen-fold of said quaternizing agent.
- 7. A method according to claim 6 wherein said step is carried out using less than ten-fold of said quaternizing agent.
- 8. A method according to claim 6 wherein said step is carried out using from five-fold to ten-fold of said quaternizing agent.
- 9. A method according to claim 8 wherein said quaternizing agent is selected from the group consisting of methyl iodide, methyl tosylate, and dimethyl sulfate.
- 10. A method for preparing a cross-bridged macropolycycle according to claim 1 comprising a series of steps of derivatizing cyclam or a particular acyclic tetraamine including a step of reducing a diquaternized intermediate, wherein said step is carried out using an amount less than fifteen-fold of reducing agent.
- 11. A method for preparing a cross-bridged macropolycycle comprising a series of steps of derivatizing cyclam or a particular acyclic tetraamine including a step of reducing a diquaternized intermediate, wherein said step is carried out using an amount of less than fifteen-fold of reducing agent.
- 12. A method according to claim 11 wherein said reducing agent is a non-catalytic reducing agent.
- 13. A method according to claim 12 wherein said reducing agent is a hydride compound.
- 14. A method according to claim 13 wherein said hydride compound is a borohydride.
- 15. A method according to claim 14 wherein said borohydride compound is selected from the group consisting of sodium borohydride and potassium borohydride.
- 16. A method according to claim 15 wherein said borohydride compound is potassium borohydride.
- 17. A method for preparing a cross-bridged macropolycycle, said method comprising derivatizing cyclam or a particular acyclic tetraamine by a series of steps including:
quaternizing an intermediate using a quaternizing agent, wherein said step is carried out using less than fifteen-fold of said quaternizing agent; and reducing a diquaternized intermediate, wherein said step is carried out using an amount of less than fifteen-fold of reducing agent; and wherein further said series of steps is carried out using one solvent system.
- 18. A method according to claim 17, carried out in the absence of any step of vacuum distilling an intermediate.
- 19. A method according to claim 17, carried out at or below 50° C.
- 20. A method according to claim 17, wherein said quaternization and reduction steps are carried out at the temperatures of from ambient temperature to 50° C.
- 21. A method according to claim 17 wherein all of said steps are carried out at concentrations of the reactants of 7% or higher in total of the sum of reactants plus solvent.
- 22. A method according to claim 17 wherein all of said steps are carried out at concentrations of the reactants exceeding 15% in total of the sum of reactants plus solvent.
- 23. A method according to claim 14 in which sodium ion is substantially absent.
- 24. A method for producing a complex of Mn and a cross-bridged macropolycyclic ligand, said method comprising reacting with manganous chloride a cross-bridged macropolycycle.
- 25. A method for producing a complex of Mn and a cross-bridged macropolycyclic ligand, said method comprising reacting a cross-bridged macropolycycle with MnCl2 which has been produced by an anhydrous reaction of manganese metal with a chlorinating agent.
- 26. A method according to claim 24, conducted in a nonaqueous solvent.
- 27. A method according to claim 25, conducted in a nonaqueous solvent.
- 28. A method for preparing a transition metal complex of a cross-bridged macropolycycle comprising
a series of steps of
(A) forming a bisaminal from an acyclic amine; (B) forming a diquat derivative of said bisaminal; (C) reducing said diquat derivative; (D) separating reducing agent and solvent from the product of step (C) in one or more operations; (E) removing residual hydride from the product of (D); (F) isolating a cross-bridged tetraazamacrocycle product of steps (A)-(E); and (G) reacting the product of step (F) with a transition-metal, thereby forming a transition-metal complex useful as a catalyst in detergent compositions.
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This is a continuation under 35 USC §120 of U.S. application Ser. No. 09/380,675, filed Sep. 7, 1999 of which in turn claims priority under 37 U.S.C. §371 to PCT International Application Serial No. PCT/IB98/00299, filed Mar. 6, 1998 which claims priority under 37 USC §119(e) to U.S. Provisional Application Serial No. 60/039,920, filed Mar. 7, 1997).
Provisional Applications (1)
|
Number |
Date |
Country |
|
60039920 |
Mar 1997 |
US |
Continuations (1)
|
Number |
Date |
Country |
Parent |
09380675 |
Sep 1999 |
US |
Child |
09832579 |
Apr 2001 |
US |